LC-MS/MS测定大鼠血浆中虎杖苷浓度  

Determination of polydatin in rats plasma by LC-MS/MS

作　　者：丁雪鹰[1] 侯晓丽[2] 孙铭学[3] 肖凯[3] 

机构地区：[1]第二军医大学药学院药剂学教研室,上海200433 [2]第二军医大学海医系毒药物研究室,上海200433 [3]第二军医大学海医系毒物药物研究室,上海200433

出　　处：《药学实践杂志》2012年第1期45-48,共4页Journal of Pharmaceutical Practice

基　　金：上海市科委中药现代化项目(08DZ1971504);国家自然科学基金(20872179;30472141)

摘　　要：目的建立测定大鼠血浆中虎杖苷浓度的LC-MS/MS方法。方法采用LC-MS/MS测定大鼠血浆中虎杖苷的浓度,以二苯乙烯苷为内标,血浆样品用乙腈沉淀蛋白,色谱柱为Agilent Zorbax SB-C18(100 mm×2.1 mm,3.5μm),流动相为甲醇-乙腈-0.1%甲酸水溶液(18∶15∶67),流速0.3 ml/min,柱温30℃。结果虎杖苷的线性范围为1.0～5 000.0 ng/ml(r=0.998 4),最低定量检测浓度为1.0 ng/ml(S/N>10),提取回收率>78%,日内和日间RSD<15%。结论本法操作简单,选择性好,灵敏度高,费时少,适用于虎杖苷在大鼠体内的药代动力学研究。Objective To estahlish a LC-MS/MS method for determination of polydatin concentration in rats plasma. Meth- ods The plasma concentration of polydatin was determined by LC-MS/MS. Using stilbene glueoside as internal standard, after pre- cipitation of the plasma proteins with methanol, the analytes were separated on an agilent zorbax SB-C18 reversed-phase column with methanol- aeetonitrile- 0.1% formic acid （18 ： 15 ： 67, v/v） and detected by eletrospray ionization （ESI） mass spectrometry in negative multiple reaction monitoring （MRM） mode. The flow rate was 0.3 ml/min. Column temperature was maintained at 30 ℃. Results The calibration curves with good linearity （ r = 0. 998 4 for plasma sample） were obtained in the range of 1.0 - 5000.0 ng/ml for polydatin. The lower limit of quantification （LLOQ） was 1.0 ng/ml. Reeoveries were around 78% for the extraction from rats plas- ma, and good precision and accuracy were aehieved. The intra-day and inter-day RSD were both less than 15.0%. This method was feasible for the evaluation of pharmacokiuetic profiles of polydatin in rats. Conclusion This method was simple, selective and sensitive. It＇s suitable for the pharmaeokinetic research of polydatin in rats plasma.

关 键 词：虎杖苷 LC-MS/MS 血药浓度 

分 类 号：R284.1[医药卫生—中药学] R917[医药卫生—中医学]